SE447369B - PROCEDURE FOR THE PREPARATION OF PHOSPHIDS OF ALUMINUM OR MAGNESIUM - Google Patents

Description

447 369 is in the form of powder or barley and if the yellow phosphorus is added slowly in liquid form. It is also advantageous if the reaction mixture is stirred mechanically during the reaction.

By the process according to the invention it is possible to produce the phosphides from aluminum or magnesium or a mixture of these phosphides in large quantities without risk and with the closest theoretical yield. The process is very environmentally friendly as hardly any by-products are formed. In addition, the metal phosphides formed do not contain significant amounts of polyphosphides. This has an effect on the subsequent use of these metal phosphides in pesticides by hydrolyzing them to produce essentially only phosphorus hydrogen which is not self-igniting in air, but hardly higher phosphides, such as diphosphane, which are self-igniting.

The elements chlorine, bromine, iodine or their hydrogen, ammonium, sulfur, phosphorus, zinc, aluminum or magnesium compounds used in the process according to the invention as catalysts, such as HCl, NH4Cl, SC12, SOCl2, SO2Cl2, PCl3, PBI3 , PJ3, PC15, PZJ4, POCl3, ZnCl2, Znßrz, AlCl3, AlBr3, MgCl2, MgBr2 or MgJ2, are suitably used in such an amount that the weight ratio of the metal to be reacted to the catalyst is substantially in the range to 10000: 200.

According to a particularly preferred embodiment of the process according to the invention, the finely powdered or granular metal is first mixed intimately with the catalyst. The mixture is heated in a suitable, sealable reactor in an inert gas atmosphere, for example under nitrogen, at normal pressure to the reaction temperature between 300 and 600 ° C. When the desired reaction temperature is reached, liquid yellow phosphorus is added at such a rate that the heat of reaction released is easily removed and the temperature is kept in the range between 300 and 100 ° C.

Under these conditions, the reaction can be easily controlled and the metal used does not melt. When the required amount of phosphorus has been added, an often reaction time of 447,369 of suitable duration is suitably maintained to enable as complete a conversion as possible. Even during the post-reaction time, the temperature is kept in the range between 300 and 60006. When the reaction is completed, the reaction product is taken out under inert gas through an outlet device arranged below the reactor in a hot state.

The invention is described in more detail with the following working examples.

Example 1. 200 g of magnesium granules are heated under nitrogen with 0.8 g of iodine in a reaction vessel heated to 35 DEG C. with an aqueous solution.

The heating is stopped and 157 g of yellow phosphorus are blended into the reaction mixture in liquid form so slowly that the temperature does not rise above 50 ° C. The delivery time is about 30 minutes.

The gray granular product can be removed from the reactor without difficulty.

Yield: 356 g; content of Mg3P2: 89%.

Example 2. 400 g of magnesium granules are heated in a reaction vessel closed with a water source under nitrogen by mechanical stirring to 300 ° C. In a dropping funnel, 320 g of yellow phosphorus and 3 g of iodine are mixed and heated to 5 ° C. The phosphorus-iodine mixture is slowly added to the heated metal. Delivery time: about 25 minutes. The temperature rises to 51 ° C. In Yield: 715 g; content of Mg3P2: 94.5%.

Exemoel 3. 200 g of magnesium granules are mixed under nitrogen with 1 g of diphosphorus tetraiodide in a reaction vessel closed with a water source and heated to 360 ° C. After the heating is completed, 162 g of liquid yellow phosphorus are added so slowly that the temperature does not rise above 50 ° C. Delivery time: about 25 minutes. The gray, granular product can be removed from the reactor without difficulty.

Yield: 361 g; content of Mg3P2: 95.5%. 447 369 âgemgel 4. 100 g of magnesium granules are mixed under nitrogen with 3 g of bromine in a reaction vessel closed with a water source and heated to 300 ° C. After the heating is completed, 80 g of liquid yellow phosphorus are slowly added to the reaction mixture. The temperature does not rise above 480 ° C. Delivery time: about 35 minutes. ¿The gray, granular product can be easily shaken out of the reactor.

Yield: 178 g; content of Mg3P2: 89%.

Example 5. g of magnesium granules is heated under nitrogen in a reaction vessel closed with a water source to 320 ° C. After the heating is stopped, a liquid mixture of 24 g of yellow phosphorus and 0.3 g of bromine is slowly added to the reaction vessel. The temperature does not rise above 390 ° C. Delivery time: 20 minutes. The reaction mixture is kept for a further 20 minutes at 380 ° C, after which the granular product can be shaken out of the reactor without difficulty. Yield: 54 g; content of Mg3P2: 87%.

Example gel 6. kg of magnesium granules is mixed with 40 g of iodine in a reaction vessel closed with a water reservoir and heated to 35006. After the heating is stopped, 8.5 kg of liquid yellow phosphorus are slowly added to the reaction mixture. During the addition, the temperature does not rise above 48,000. The reaction mixture is stirred mechanically throughout the reaction time. Delivery time: 70 minutes.

The gray, granular product is removed at the bottom through an opening without further opening the reactor.

Yield: 18.4 kg; content of Mg3P2: 95%.

Example gel 7. 100 g of magnesium-aluminum alloy (50% magnesium, 50% aluminum) are mixed in a reaction vessel closed with a water source under nitrogen with 2 g of bromine and heated to 33 ° C. after the heating is stopped, 100 g of liquid yellow phosphorus are slowly added to the reaction mixture. The temperature does not rise above. 447 369 45OOC. Delivery time: about 30 minutes. The gray, granular product can be easily removed from the reactor.

Yield: 200 g; content of magnesium phosphide and aluminum phosphide: 95%. Example 8. 1.5 kg of magnesium-aluminum alloy (50% magnesium, 50% aluminum) are mixed under nitrogen with 15 g of iodine in a reaction vessel closed with a water source and heated to 36 DEG C. After the heating is stopped, 1.5 kg of liquid yellow phosphorus are slowly added to the reaction mixture. The temperature does not rise above 450 ° C. Delivery time: 30 minutes. The gray, granular product can be easily removed from the reactor.

Yield: 2.9 kg; content of magnesium phosphide and aluminum phosphide: 90%.

Example 9. 64 g of aluminum granules are mixed under nitrogen with 1 g of iodine in a reaction vessel closed with a water source and heated to 38 ° C. After the heating is stopped, 62 g of liquid yellow phosphorus are slowly added. The temperature does not rise above SOOOC. Delivery time: about 30 minutes. The gray, granular product can be easily removed from the reactor.

Q Yield: 122 g; content of aluminum phosphide: 85 a.

Claims (6)

v '447 369 PATENT CLAIMS: 1. A process for the production of aluminum or magnesium phosphides by reacting finely divided metal or alloying the two metals with phosphorus, Esa may know from the fact that the metal is reacted with yellow at a temperature between 306 and 600 ° C. phosphorus in an inert gas atmosphere and in the presence of chlorine, bromine, iodine or a combination of these elements with phosphorus, sulfur, hydrogen, ammonium, zinc or the metal to be reacted, such as catalysts. 2. A process according to claim 1, characterized in that the catalyst is mixed with the metal before the reaction. in 3. A process according to claim 1, characterized in that the catalyst is mixed with the yellow phosphorus before the reaction. 4. A method according to any one of claims 1-3, characterized in that the yellow phosphorus is added slowly in liquid form. 5. A process according to any one of claims L-4, characterized in that the reaction mixture is mechanically stirred during the reaction. 6. A method according to any one of claims 1-5, characterized in that the metal or alloy is used in granular form.